Upload
others
View
6
Download
0
Embed Size (px)
Citation preview
Diablo 5000A RTGA
Getting Started Manual
By Diablo Analytical, Inc.
Notices
© Diablo Analytical, Inc. 2007-
2014, All rights reserved.
No part of this manual may be reproduced in
any form or by any means (including
electronic storage and retrieval or translation
into a foreign language) without prior
agreement and written consent from Diablo
Analytical, Inc. as governed by United States
and international copyright laws.
Manual Part Number
D3163-90110
Edition
Fifth Edition, January 2014
Printed in USA
Diablo Analytical, Inc.
5141 Lone Tree Way
Antioch, CA 94531 USA
Acknowledgement of Trademarks
Microsoft®, Windows®, and Excel® are
registered trademarks of Microsoft
Corporation. Agilent®, MassHunter® and ChemStation® are registered trademarks of
Agilent Technologies, Inc.
Warranty
The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions. Further, to the maximum extent permitted by applicable law, Diablo disclaims all warranties, either express or implied, with regard to this manual and any information contained herein, including but not limited to the implied warranties of merchantability and fitness for a particular purpose. Diablo shall not be liable for errors or for incidental or consequential damages in connection with the furnishing, use, or performance of this document or of any information contained herein. Should Diablo and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate agreement shall control.
Technology Licenses
The hardware and/or software described in
this document are furnished under a license
and may be used or copied only in
accordance with the terms of such license.
Restricted Rights Legend
If software is for use in the performance of a
U.S. Government prime contract or
subcontract, Software is delivered and
licensed as “Commercial computer
software” as defined in DFAR 252.227-7014
(June 1995), or as a “commercial item” as
defined in FAR 2.101 (a) or as “Restricted
computer software” as defined in FAR
52.227-19 (June1987) or any equivalent
agency regulation or contract clause. Use,
duplication or disclosure of Software is
subject to Diablo Analytical’s standard
commercial license terms, and non-DOD
Departments and Agencies of the U.S.
Government will receive no greater than
Restricted Rights as defined in FAR 52.227-
19(c)(1-2) (June
1987). U.S. Government users will receive no greater than Limited Rights as defined in FAR 52.227-14 (June 1987) or DFAR 252.227-7015 (b)(2) (November 1995), as applicable in any technical data.
Safety Notices
CAUTION
A CAUTION notice
denotes a hazard. It calls
attention to an operating
procedure, practice, or
the like that, if not
correctly performed or
adhered to, could result in
damage to the product or
loss of important data. Do
not proceed beyond a
CAUTION notice until the
indicated conditions are
fully understood and met.
WARNING
A WARNING notice
denotes a hazard. It calls
attention to an operating
procedure, practice, or
the like that, if not
correctly per-formed or
adhered to, could result
in personal injury or
death. Do not proceed
beyond a WARNING
notice until the indicated
conditions are fully
understood and met.
Diablo 5000A RTGA Getting Started Manual Contents iii
Contents
Getting Started 1
Overview ................................................................................................................................... 1
Installation 2
System Installation ..................................................................................................................... 2 Support....................................................................................................................................... 2 MSD ChemStation or MassHunter Acquisition Software ......................................................... 2
Verify the MSD ChemStation or MassHunter GC/MS Installation ............................ 3 MS Sensor Software .................................................................................................................. 3
Theory of Operation 4
Setting up the Hardware 5
Connecting sample lines ............................................................................................................ 5 Changing Orifice Disks ............................................................................................................. 6 Temperature controller operation and maintenance ................................................................... 8
Watlow EZ-Zone Controller ........................................................................................ 8 Pressure sensor operation and maintenance ............................................................................... 9
To connect the pressure sensor to the cross ................................................................. 9 To connect the pressure sensor controller to the PC .................................................. 10 To configure the pressure sensor controller:.............................................................. 10 To zero the pressure sensor: ...................................................................................... 10
Special Hardware Considerations ............................................................................................ 11 MSD Configuration for low-mass (hydrogen) detection ........................................... 11 Converting the MSD from RTGA to GC/MS ............................................................ 11
Setting MS Sensor System Options 12
Starting the MS Sensor software ............................................................................................. 12 Configuring the MS Sensor software ....................................................................................... 13
Creating a Method 14
Introduction to creating MS Sensor Methods .......................................................................... 14 Method components ................................................................................................................. 15
Instruments components ............................................................................................ 16 Tuning the RTGA Mass Spectrometer ...................................................................... 17 Add the additional instruments (e.g., the pressure transducer) .................................. 18 Signals components ................................................................................................... 18 Calculations component (optional) ............................................................................ 19 Data channels component .......................................................................................... 21 Process monitoring parameters .................................................................................. 22 Completing the method ............................................................................................. 23
iv Contents Diablo 5000A RTGA Getting Started Manual
Acquiring Data 24
Preparation ............................................................................................................................... 24 Start the run ............................................................................................................................. 26 Stop the run and view the results ............................................................................................. 27
Troubleshooting 27
Evaluating RTGA Interface Performance ................................................................................ 27
Index 29
Diablo 5000A RTGA Getting Started Manual Getting Started 1
Getting Started
Overview
The Diablo Analytical 5000A Real-Time Gas Analyzer (RTGA) monitors gaseous
process streams and produces trend plots and Excel-compatible data files.
The hardware consists of:
An Agilent Technologies 5975 or 5977 Mass Selective Detector (MSD),
with the Real-Time Gas Analyzer hardware interface
A custom Watlow EZ-Zone temperature controller with a custom thermal
jacket for the interface
An MKS PDR2000 Controller with a high-performance capacitance
manometer pressure sensor
A vacuum isolation valve
Associated plumbing
A personal computer (PC), as described on the next page
The analyzer is controlled by the Agilent MSD ChemStation software or MassHunter
GC/MS Acquisition software. Method creation and data processing are done by the
Diablo MS Sensor 3.0 software. Both programs run on a personal computer (PC).
2 Installation Diablo 5000A RTGA Getting Started Manual
Installation
System Installation
Diablo Analytical personnel or an authorized representative will install the 5000A
RTGA hardware and software and will also check out the entire system. The
information on this page is provided to the user for future reference.
Support Agilent Technologies provides warranty service and support for the 5975 or 5977
MSD and ChemStation or MassHunter computer system. Diablo Analytical provides
warranty service and support for the D3163A RTGA kits. Contact Diablo Analytical
if you have any questions about the operation of your RTGA system.
Diablo Analytical, Inc. 5141 Lone Tree Way
Antioch, CA 94531
Phone: (925) 755-1005
Fax: (925) 755-1007
E-mail: [email protected]
Web: http://www.diabloanalytical.com
MSD ChemStation or MassHunter Acquisition Software
For Agilent 5975 MSDs controlled by the MSD ChemStation Software
See the MSD ChemStation documentation for the installation procedure. The MSD
ChemStation software, including the IO Libraries, must be correctly installed and
configured before running the MS Sensor software. The ChemStation software
revision must be G1701 DA (D.00.00.38) or higher.
For Agilent 5975 or 5977 MSDS controlled by the MassHunter Acquisition Software
See the MassHunter GC/MS Acquisition documentation for the installation
procedure. The MassHunter Acquisition software must be correctly installed and
configured before running the MS Sensor software. The MassHunter GC/MS
Acquisition software revision must be B.07.00 SP1 or later.
Important: The MSD ChemStation or MassHunter GC/MS Acquisition software must be closed before starting the MS Sensor Software.
Diablo 5000A RTGA Getting Started Manual Installation 3
Verify the MSD ChemStation or MassHunter GC/MS Installation
Before attempting to acquire data from a 5975 or 5977 MSD with the MS Sensor
Software, you should verify that the MSD ChemStation or MassHunter GC/MS data
system is configured correctly by performing a standard autotune.
MS Sensor Software
Before installing the Real Time Gas Analyzer MS Sensor software, read the
document release notes.htm in the root directory of the MS Sensor CD-ROM. This
document contains installation and usage information that may not be included in the
software manual or help file.
The MS Sensor Software Reference Manual is also provided on the CD-ROM. The
reference manual provides more detailed information on how to use the MS Sensor
software than is included in this Getting Started Manual.
To begin installation, run the program setup.exe in the root directory of the MS
Sensor software CD-ROM. Follow the on-screen instructions.
4 Theory of Operation Diablo 5000A RTGA Getting Started Manual
Theory of Operation
The sample interface for the Real Time Gas Analyzer is shown in Figure 1.
To RV12 pump
To
MSD
(10-6 Torr)
Pressure
Transducer Process
Stream in
Out to
vent
Molecular flow
Orifice 50
Sonic Flow
Orifice 30
Isolation
Valve
..
[RS232 interface]
Minimum
40ml/min flow
(350 for trace)
~0.5
TorrSample Tee
Sample
Orifice
HV
Orifice
To RV12 pump
To
MSD
(10-6 Torr)
Pressure
Transducer Process
Stream in
Out to
vent
Molecular flow
Orifice 50Orifice 50
Sonic Flow
Orifice 30Orifice 30
Isolation
Valve
....
[RS232 interface]
Minimum
40ml/min flow
(350 for trace)
~0.5
TorrSample Tee
Sample
Orifice
HV
Orifice
Figure 1: The 5000A RTGA sampling interface.
The interface consists of a sampling tee and a sampling cross. Sample input tubing
is connected to the top of the sampling tee. One branch of the tee is connected to the
sampling cross through a sample orifice, while the other is a vent line for excess
sample. Since only a small fraction of the sample input will flow through the sample
orifice into the sampling cross, the bulk of the sample can be routed back into the
process, if desired, or vented.
A fixed orifice (30 µm i.d.) limits the amount of sample that is drawn. The first
orifice (the sample orifice) is in between the sampling tee and the sampling cross.
One branch of the cross connects to the large “bypass” vacuum pump (Pfeifer DUO-
10M, Edwards RV12, or Edwards nXDS-10i). This pump reduces the pressure in the
cross and pulls the majority of the sampled stream out to waste.
A second leg on the cross allows a precision pressure transducer to read the cross
pressure. This signal can be used to adjust the data for changes in sample pressure.
The final branch contains a second orifice (the high vacuum orifice) that further
limits the amount of sample reaching the mass spectrometer and allows the mass
Diablo 5000A RTGA Getting Started Manual Setting up the Hardware 5
spectrometer to maintain the necessary high vacuum (typically 1x10-6 Torr). The
default orifice diameter is 50 µm for this stage.
Flow then passes through a vacuum isolation valve that is useful for troubleshooting
and maintenance. The outlet of the isolation valve connects to the mass spectrometer
interface and directs the sampled stream to the ionization region in the mass
spectrometer.
The two orifices and the large vacuum pump allow the high-vacuum mass
spectrometer to sample a gaseous input directly with minimal dwell time. A thermal
jacket envelopes the sampling tee and the cross to maintain the desired sample
temperature until high vacuum is encountered. The Watlow EZ-Zone temperature
controller regulates this temperature to the user-selected set point.
If excess sample is to be vented, it is recommended that some length of tubing be
attached to the outlet of the sample tee to limit back diffusion of air into the cross.
Setting up the Hardware
Connecting sample lines
Caution: Particulates and condensed liquids or droplets in the sample stream can plug the 30-μm sample orifice, which will then need to be replaced. It is the responsibility of the user to ensure that their sampling system is designed to eliminate particulate and liquid prior to the sample gas stream reaching the RTGA sampling tee.
The sample input and output connections are standard 1/16-inch Swagelok fittings.
By using 1/16-inch tubing, the dwell time of the sample line can be minimized
without introducing a large pressure drop. The sample input is connected to the top
of the interface and the vent or process return is connected to the bottom of the
interface. To make a new fitting connection, make sure the tube is fully inserted into
the fitting body. Finger-tighten the fitting and then tighten ¾ of a turn with a 5/16-
inch wrench on the compression nut and a 5/16-inch wrench on the adapter body.
6 Setting up the Hardware Diablo 5000A RTGA Getting Started Manual
Figure 2: A photograph of the RTGA interface with the sampling tee identified.
If necessary, user-supplied fittings can be used to adapt process lines to the 1/16 inch
required for the interface. Heating the sample lines is the responsibility of the user.
Changing Orifice Disks
The RTGA uses two laser-drilled orifice disks to provide pressure reduction in the
sampling interface. The orifice disks that are supplied with the RTGA are listed in
Table 1. Note that orifice disks with other diameters are available for special
applications.
Table 1: Orifice disks included with the 5000A RTGA.
*The default orifice configuration Installed in the interface at the factory.
Important: Due to the nature of the seal produced by the VCR fitting, the orifice disks cannot be reused. Replacement orifice disks can be purchased from Diablo Analytical.
Orifice Diameter (μm)
Description Part Number
30* Standard sample orifice D3163-20500
50* Standard high vacuum orifice D3163-20510
350 Special high vacuum orifice for trace
analysis.
D3163-20550
Diablo 5000A RTGA Getting Started Manual Setting up the Hardware 7
Figure 3: A photograph of the RTGA interface with the VCR fittings containing the
sample and high-vacuum orifice disks identified.
The standard factory orifice configuration is applicable to a broad range of
applications. However, either orifice disk can be easily replaced using the following
procedure.
1. Close the isolation valve to the MSD.
2. Note the current interface pressure, and then unplug the power cord to the MKS
PDR 2000 pressure controller.
3. Turn off the bypass sampling pump.
4. Loosen the VCR fitting that contains the orifice disk that you want to change.
The orifice disk is used as the seal in the VCR fitting. You will need two open-
end wrenches: 3/4" and 5/8". Once you have unscrewed and separated the two
nuts, you can pull them away from each other and expose the orifice disc, which
will be sandwiched between the two ends of the fittings.
5. Remove the old orifice from between the fittings. It is possible you may have to
loosen the screw that attaches the interface bracket to the side of the MSD in
order to separate the two fittings far enough for the orifice to be removed.
6. Insert the new orifice disk in between the two fittings - use gloves to handle the
orifice so that you don't get fingerprints on the surface. This step can be a little
tricky, and it sometimes helps to place the orifice inside the large hex nut first,
and the slide it over the fittings.
7. Re-tighten the two nuts - you should hold the large nut stationary while
tightening the small nut. You can use the small hole drilled in the side of the
large nut to confirm that the orifice is in place and didn't drop out. Don't over
tighten the VCR fittings - tighten it 1/8 turn past finger tight.
8. If you loosened the interface bracket screw, re-tighten it.
9. Turn the bypass pump back on.
10. Plug the power cord back into the pressure controller and wait for the reading to
stabilize. Make sure that the interface returns to a similar vacuum pressure as
before.
11. Open the isolation valve and perform an autotune and check for leaks.
8 Setting up the Hardware Diablo 5000A RTGA Getting Started Manual
Temperature controller operation and maintenance
The 5000A RTGA is shipped with a custom temperature controller console using a
Watlow EZ-Zone Controller.
Caution: The maximum temperature for the interface is 200 °C. Do not enter values higher than this into the controller. It is possible damage the heater blanket and/or the MSD electronics if you use interface temperatures higher than 200 °C!
Watlow EZ-Zone Controller
Figure 5: The front panel of the Watlow EZ-Zone Temperature Controller.
Changing the interface temperature
Simply press the gray up/down arrows on the right side of the temperature controller
to adjust the interface temperature set point. The upper numeric display shows the
actual interface temperature, while the lower numeric display shows the current set
point.
Setting the Temperature Display Units
Note: The temperature controller is set to units of ºC at the factory.
Use the following procedure to set the units of the displayed temperature (ºC or ºF).
Refer to Figure 5.
1. Press and hold both of the gray up/down arrow buttons for approximately 6
seconds until the controller shows “A1” in the top display, and “SEt” in the
bottom display. Note that you will have to continue to hold the buttons after
“oPEr” appears in the lower display.
2. Press the down arrow key until the top display reads “9LbL” (for global). The
bottom display should still read “SEt”
Diablo 5000A RTGA Getting Started Manual Setting up the Hardware 9
3. Press the green advance button until “C_F” is in the bottom display.
4. Press the gray up arrow key until the desired temperature units are shown in the
top display (“C” or “F”).
5. Press the gray infinity key (“∞”) until you reach the “home” display with the
actual temperature in the top display and the set point in the lower display.
Auto-tuning the controller
Note: The temperature controller is auto-tuned at the factory at a temperature of 120
ºC.
If the actual temperature does not stabilize at the set point or significantly overshoots
or undershoots the set point, it may be necessary to “tune” the controller using the
autotune function. Please refer to Figure 5.
1. Start with the temperature controller off and the interface and heater blanket
cold. In addition, it is important to make sure that the heater blanket is tightly
secured and in good contact with the RTGA interface.
2. Turn on the temperature controller and press the up/down arrow buttons to select
the desired interface temperature set point.
3. Press the green advance button until the bottom display reads “AUt 1”.
4. Press the up arrow button until the top display reads “Yes” then press the
infinity button to return to the temperature display.
5. The unit should begin autotuning. The upper display will flash between “tUn 1”
and the actual temperature until the autotune is complete.
Caution: During autotuning, the controller will cycle the temperature around a value of 90% of the current temperature set point. Consequently, you should be careful not to tune at a set point that results in the temperature cycling above 200 °C.
Pressure sensor operation and maintenance
To connect the pressure sensor to the cross
Note: This procedure is normally performed at the factory during assembly of the
interface.
The pressure sensor is connected to the sampling cross with standard VCR4 fittings.
To install a new pressure sensor, loosen the cap fitting with a 5/8- and 3/4-inch or
adjustable wrenches. Use the lint-free gloves included with the MSD ship kit to
handle the VCR4 gasket. Carefully place the gasket on top of the cross fitting and
place the pressure sensor on top of the gasket. This is best done if the female fitting
on the pressure sensor is slid back to allow the sealing surfaces to meet. Finger-
tighten the male and female nut assemblies. Using the wrenches, tighten the fittings
an additional 1/8 of a turn.
10 Setting up the Hardware Diablo 5000A RTGA Getting Started Manual
To connect the pressure sensor controller to the PC
Two cables are included with the MKS PDR 2000 pressure sensor controller. One
(part no. CB628S-3-10) is for connecting the sensor to the controller while the other
(part no. CBPDR-1-10) is for connecting the controller to the PC. An appropriate
power cord is also included for the sensor controller.
To configure the pressure sensor controller:
The controller has no On/Off switch so, once it is plugged in, the LED display will
light and begin to flash. To obtain accurate readings, the PDR 2000 Controller needs
to be configured for the sensor in terms of units, full scale, and zero.
1 To begin configuration, press the [Select] button on the controller. The display
will flash OFF and the LED indicator will be on SetPt1 Hi.
2 Press [Select] four times so that Units is indicated. Use the [Raise] and [Lower]
buttons to scroll through the options until torr is shown. Press [Select] to choose
torr; the controller will advance to the Calibrate option.
3 Press [Select] again to move to the Full Scale option. Make sure that the
controller is set to the pressure sensor channel (CH1 or CH2, CH1 preferred),
then use [Raise] and [Lower] to set the full scale value to that of the sensor. For
the sensor supplied with the RTGA interface, this value is 10 torr.
Figure 6: The MKS PDR2000 pressure controller.
The controller is now configured and ready to be zeroed.
To zero the pressure sensor:
Note: The pressure transducer is zeroed at the factory. You should only re-zero the
sensor if you are certain that the calibration has drifted.
Important: Do not zero the pressure sensor if there is a leak anywhere in the
interface assembly.
To check the current zero setting, make sure that the roughing pump for the interface
is on. Close the isolation valve to the mass spectrometer and plug the sample input
and output branches on the sampling tee. Allow the roughing pump to run for at least
15 minutes.
Important: The pressure should have been powered and heating for at least 4 hours
before attempting to zero the signal.
Diablo 5000A RTGA Getting Started Manual Setting up the Hardware 11
The pressure sensor can be zeroed in two places. A zero adjustment is located on the
transducer itself and can be turned with a small flat-blade screwdriver. Zeroing can
also be done on the controller front panel. Make sure that the channel selection is on
the pressure sensor to be zeroed (typically CH 1). Press the [Select] button until the
Zero LED is lit. Using the [Raise] and [Lower] buttons, adjust the readout to 0.000
torr.
If the sensor still cannot be zeroed, please refer to the MKS manual included with
your system.
Important: If either component (pressure sensor or controller) is replaced, the system will need to be re-zeroed.
Special Hardware Considerations
MSD Configuration for low-mass (hydrogen) detection
The standard Agilent 5975/77 MSD is not designed to detect low-mass species like
Hydrogen or Helium since these species are typically the carrier gases used in
GC/MS applications. In order to detect low-mass ions, the MSD ionization source
must be modified to use a special low-gauss magnet and an ultra-wide draw-out
plate. These parts are included with the 5000A RTGA kit and may have been
installed in the MSD at the factory or onsite during installation of the RTGA system.
You can confirm this by reviewing the Installation and Configuration Data Sheet
that was provided with the RTGA documentation. If you have any questions about
the configuration of your RTGA as it was shipped form the factory, please contact
Diablo Analytical.
Converting the MSD from RTGA to GC/MS
The Agilent 5975/77 MSD used in the Diablo 5000A RTGA can also be used in a
standard GC/MS configuration by adding the appropriate Agilent Technologies Gas
Chromatograph. To convert from RTGA operation to GC/MS operation, you simply
vent the MSD, remove the RTGA interface assembly from the MSD and replace it
with the standard GC/MS interface that is included with the system. Please contact
Diablo Analytical for more information on reconfiguring your RTGA for use as a
standard GC/MS.
12 Setting MS Sensor System Options Diablo 5000A RTGA Getting Started Manual
Setting MS Sensor System Options
Starting the MS Sensor software
The Diablo MS Sensor software is used to acquire and display continuous process
results in the form of real-time trend plots and data tables.
The MS Sensor software requires the Agilent Technologies MSD ChemStation or
MassHunter Acquisition software to control the Agilent Technologies 5975 or 5977
MSD. However, the MS Sensor software acts as a simplified operator interface to
the MSD ChemStation or MassHunter software. In most applications, the user will
only need to interact with the MS Sensor software.
Important: The MSD ChemStation or MassHunter Acquisition software must be installed and configured before starting the MS Sensor software. Refer to the MS Sensor manual for more information on advanced topics such as the Method Wizard, a simplified user interface for quickly creating new methods.
To start the MS Sensor software, double-click the MS Sensor icon on the desktop or
run C:\MSSensor\MSSensor.exe. The main window and the current event log appear
(Figure 7).
Diablo 5000A RTGA Getting Started Manual Setting MS Sensor System Options 13
Figure 7: The main screen of the MS Sensor software.
Configuring the MS Sensor software
To configure the MS Sensor software, select Tools/Options from the menu at the top
of the screen. The Options dialog box appears (Figure 8).
Figure 8: The MS Sensor System Options dialog box.
1. Set the root method directory: select “Browse” and choose a directory for
storing methods. The default directory is C:\MSSensor\methods. The user can
choose to put methods in a more convenient place if desired.
2. Set the default data directory: select “Browse” and specify the path to the data
directory for storing data folders. It is best to place the data directory on the
14 Creating a Method Diablo 5000A RTGA Getting Started Manual
same drive as the MSD ChemStation software that controls your Agilent 5973
MSD.
3. At the bottom of the window, the user can select a default program, such as
Notepad or Excel, to open the data text file. If the user has specified that an
application will use CSV files, it will launch that application when the file is
accessed. In addition, the user can select the Use the specified application and
browse to find the executable.
Creating a Method
Introduction to creating MS Sensor Methods
All data acquisition is controlled by a method. This section describes how to create a
simple method that monitors the laboratory air.
Methods are not single files. Methods are directories named with a “.m” extension
that contain sets of “.rcp” (recipe) files. When creating a new method, the directory
is created first. The recipe files to fill that directory are created later as the user
specifies method components in the Edit Method window.
1 Run C:\MSSensor\MSSensor.exe to start the software. For ease of use, we
suggest creating a shortcut icon on the desktop to do this. The installation
program normally does this for you.
2 Select [Method/New] from the menu at the top of the screen. The Method
Directory Specification screen appears (Figure 9).
Figure 9: The method selection dialog box.
Diablo 5000A RTGA Getting Started Manual Creating a Method 15
3 Type a name in the Selected Method field. For this example, we suggest the
name Roomair.
4 Select OK to create the new method directory and close the dialog box. The Edit
Method window opens (Figure 10).
Figure 10: The method-editing screen.
Method components
A method consists of five components, which are created in the order shown in Table
2.
Component Description
Instruments Instruments are signal-generating devices such as the Agilent 5975 or
5977 MSD. Instruments can be added, deleted, or edited. The user must
choose the instrument(s) to be used to acquire data and subsequently
configure the selected instrument(s).
Signals Signals are the numeric data values obtained from the various
instruments. Some instruments only generate a single signal (e.g.,
pressure) whereas others can generate multiple signals (e.g., MSD).
Define the specific signals wanted here. In addition, a simple linear
calibration for raw signal response can be defined by the user and
applied directly to the raw signal.
Calculations In the calculations section, one can define mathematical functions to
apply to signal values. Calculations can contain one or more signal
values as well as constants, mathematical operators, and mathematical
functions. An example is to apply a non-linear calibration function to a
signal that displays a non-linear response over the concentration range
of interest.
Data Channels Data channels are the final calculations that create real-time trend plots
and tables. This component applies a second user-defined equation,
which can contain calculation results, signal values, constants,
mathematical operators, and mathematical functions. While a
calculation applies to a specific signal from a specific instrument, data
channels can combine data from multiple signals and instruments.
Process Monitoring Parameters
This section allows the user to set the data acquisition rate, method run
time and data signals collected, and to configure the display parameters for the data plots.
16 Creating a Method Diablo 5000A RTGA Getting Started Manual
Table 2: A summary of MS Sensor method components.
Instruments components
Instruments components are created first. They define the source (or sources) of the
signals. A method can, and usually does, contain multiple instruments components.
1. If the Edit Method window is not open for Roomair.m, select
Method/Open/Roomair.m from the top screen to build the method.
2. To create an instrument, right-click the Instruments icon and select New
Instrument in the Edit Method window or select Add Instrument from the Edit
pull-down menu. The Add New Instrument dialog box appears (Figure 11).
Figure 11: The Add New Instrument dialog box.
3. The Instrument Description is the name of the instrument. Type 5975 or 5977 in
this field.
4. Select Agilent MassHunter MSD from the Instrument Type drop-down window.
Select Add and the MSD Acquisition Parameters window opens (Figure 12).
Figure 12: The Agilent MassHunter MSD Acquisition Parameters dialog box.
Add the masses desired for the method Roomair. In this case, masses 18 (water),
28 (nitrogen/carbon monoxide), 32 (oxygen), 40 (argon) and 44 (carbon dioxide)
are appropriate. The system automatically determines the mass range to scan and
puts these values in the signal selection window.
5. Click Open Tune Window to tune the RTGA.
Diablo 5000A RTGA Getting Started Manual Creating a Method 17
Tuning the RTGA Mass Spectrometer
Tuning the mass spectrometer standardizes its mass axis and relative response for a
known calibration compound. For most applications on the RTGA, particularly fuel
cell measurements, the mass spectrometer should be tuned for low molecular weight
species.
To optimize this performance, the mass spectrometer software has automated tuning
algorithms for a wide range of molecular weights (Autotune – Atune.U), low
molecular weights (Low Mass Autotune – Lomass.U), and a special tuning algorithm
for hydrogen-containing samples such as fuel cell systems (Hydrogen Tune –
HTune.U). The latter two are most useful with the RTGA.
RTGA Tuning Procedure:
1. Click the “Open Tune Window” button in the MassHunter MSD Instrument
Acquisition Parameters window. This launches the mass spectrometer tuning
and control window. For additional information about the mass spectrometer
and its operation, refer to chapter 2, “Operating the MSD” in the 5975or 5977
hardware manual. For mass spectrometer software help, click Help in the tune
window.
2. Check the system status by clicking Vacuum and selecting Vacuum/Temp
status. If the instrument is not already pumped down, click Vacuum Status and
select Pump Down. Normally the mass spectrometer will begin a pump-down
cycle automatically after initialization. The software will prompt what actions to
take and will indicate how long to let the system pump down before operation.
3. FOR NON-HYDROGEN APPLICATIONS, make sure the sample isolation
valve is in the closed position and that the mass spectrometer is pumped down
and equilibrated for at least 1 hour. In the tuning and control window, click Tune
and select Low Mass Autotune. The system will then tune the mass spectrometer
and produce a tune report at the printer.
Archive this report as it will serve as a record of instrument performance and
can be used to gauge maintenance intervals. The system is now ready to be
calibrated for non-hydrogen applications.
4. FOR HYDROGEN APPLICATIONS, make sure the sample isolation valve is
in the open position and the mass spectrometer is pumped down and equilibrated
for at least 1 hour. In addition, make sure that the DUO 10M or XDS-10
sampling pump is turned on. Connect a sample line to the top of the sampling
tee and an appropriately vented exit line to the bottom of the sample tee.
To tune the mass spectrometer for hydrogen, the sample stream should be 50 to
100% hydrogen with nitrogen the preferred balance gas. Adjust the sample flow
so that 30 to 50 mL/min is measured out the exit line.
In the tuning and control window, click Hydrogen and then select Full Hydrogen
Tune. The system will then tune the mass spectrometer and produce both a low
mass tune report and a hydrogen tune report at the printer.
Archive these reports as they will serve as a record of instrument performance
and can be used to gauge maintenance intervals. The system is now ready to be
calibrated for hydrogen applications.
Tuning should be performed when necessary and the final tune report should be
kept in a log book. Use this information to detect the start of a tuning problem
and to monitor the rise of the electron multiplier and ion focus voltages over
18 Creating a Method Diablo 5000A RTGA Getting Started Manual
time. These reports aid in planning ion source cleaning or multiplier
replacement. More information on tuning can be located in the MSD
ChemStation Help by typing tuning.
5. Save the instrument configuration.
Add the additional instruments (e.g., the pressure transducer)
Select the new instrument to be added from the pulldown menu (e.g., PDR-2000).
Select OK. Configure the new instrument as appropriate (e.g., for the PDR2000, . . .).
If a pressure transducer is included in the interface, add another instrument. Name it
(perhaps Pressure Transducer) and select the MKS PDR 2000. Select “Add” to open
another window where the COMM port can be configured.
Make sure the cables connecting the pressure controller to the pressure sensor and
the PC are correctly connected and the pressure controller has power. Once
configured, select Test to verify the connection. Click Save to exit.
Signals components
Now that instruments have been added to the method, signals must be defined and
calibrated.
1. To create the first Signals component, right-click the Signals icon and select
New Signal from the menu. The Edit Signal window opens (Figure 13).
Figure13: The signal-editing dialog box..
2. Signal Description is the name of the signal. Enter Water in the field.
3. The Instrument field specifies the instrument that will supply the signal. Select
5977 from the drop-down menu.
4. Select Mass Abundance in the Signal Type drop-down menu. In the Signal
Index Values, select 18 for m/z from the list. Refer to the MS Sensor software
manual for other signal types and usage.
5. Check the Create New Data Channel box. This will include the water signal as
one of the values to be plotted.
Diablo 5000A RTGA Getting Started Manual Creating a Method 19
6. The Linear Calibration function allows the user to enter a calibration equation
for the analyte. Alternatively, the user can select the Calibrate button, enter the
amount and signal data and the system will automatically calculate a linear
calibration equation.
The system will use a default equation with a slope of 1 and an intercept of 0 if
the user enters no information. For this test, do not change the calibration
entries.
Select Save in the Edit Signal Screen to save the changes.
7. Create additional signals for each of the other masses. In addition, create a new
signal for the total ion measurement. Name the signal Total Ion and set the
signal type to “Total Ion Signal”. The Signal index values are grayed out with
this choice since the system knows what signals to use as a source. Check the
Create a New Data Channel box and click “Save”.
8. Finally, if you have another instrument (e.g., a pressure sensor) installed on the
interface, create an additional signal for this named Pressure. Select Pressure
Transducer as the instrument and CH 1 Pressure as the Signal Type. Check the
Create a New Data Channel box and click Save.
The expanded trees in the method window should look like Figure 14.
Refer to NIST website for help in choosing m/z values.
Figure 14: The method editing tree showing the signals present in the method.
Calculations component (optional)
1. To create a new calculation, right-click the Calculation icon and select New
Calculation. The Edit Calculation window opens (Figure 15).
20 Creating a Method Diablo 5000A RTGA Getting Started Manual
Figure 15: The calculation-editing dialog box.
2. Enter an appropriate label such as Normalized Composition Total into the
Description field.
3. Click Formula and the Edit Component Formula window will appear. The
window displays all available formula elements. To include a signal component
in the formula, double-click the signal component in the list box. A small dialog
appears which allows the user to choose from the raw signal, calibrated signal,
calibration slope, or calibration intercept.
4. For this example, we will create a calculation to allow normalized percent
compositions to be determined. For this calculation, we will need a sum of all
the calibrated responses.
Double-click the Sig1: Water signal in the Components window and select the
calibrated signal response. Click OK and (Sig1.Cal) will appear in the Current
Formula window.
Click the + button in the Operators window and select the next calibrated signal.
Repeat this procedure until all of the compound signals (signals 1 - 5) are added
together (Figure 16).
Figure 16: The formula editor.
Diablo 5000A RTGA Getting Started Manual Creating a Method 21
5. Confirm the function is valid by selecting the Test button. If the calculation is
acceptable, a window will appear stating that the expression is valid.
6. Click OK on the Edit Formula screen.
7. If this signal is desired in the real time plotting, select Create New Data
Channel.
8. Save your calculation.
Data channels component
The fourth area of the method is the data channels section. The data channels are the
real-time, plotted data in the Real-Time window. A data channel can be as simple as
an unaltered signals component or something much more complex involving
multiple signals and functions
Two display options are listed at the bottom of the window (Figure 17). Display
Channel in Data Grid allows the values to be placed in a tabular format in the real-
time windows. Display Channel in Trend Plot allows multiple plot windows to be
used and signals with very dissimilar magnitudes (i.e. sample pressure and total ion)
to be placed in different plots.
In the current example, several data channels already exist. They were created when
the signals components were made. To complete the normalized composition data
for water, let’s create a new data channel by right-clicking the Data Channel icon and
selecting New channel or by clicking Edit and selecting Add Data Channel. Name
the new data channel Norm Water and click Formula.
Figure 17: The Data Channel dialog.
Formula allows the user to modify the existing formula for that data channel or
create a new formula. In the Edit Channel Formula window (Figure 18), calculation
components as well as signal components are selectable as signals. To finish the
22 Creating a Method Diablo 5000A RTGA Getting Started Manual
normalized composition signal for the water example, highlight the 0 in the constant
box, enter 100, and click Insert. This is how numerical values are entered into the
formula.
Click the multiplication sign followed by double-clicking the water signal in the
components window. Choose the signal type for water. In this case, both calibrated
signal response and raw signal response will give the same value since there is no
calibration defined for water. Next, click the divide operator and then double-click
the Normalized Components calculation signal. This will perform the required
calculation and output it to a new data channel. In this way, the user can
automatically preprocess the data before it is plotted or recorded and simplify the
data output for evaluation.
Click OK on the Formula screen and save the data channel.
Figure 18. The formula editor showing the formula for calculating normalized water
response.
Process monitoring parameters
The final section of the method deals with the process monitoring parameters. To
access these parameters, double-click the Process Monitoring Parameters tree or
select Edit Process Monitoring parameters from the menu bar. A window with four
tabs appears (Figure 19).
Diablo 5000A RTGA Getting Started Manual Creating a Method 23
Figure 19: The Process Monitoring Parameters dialog box.
The Timing tab permits the user to set acquisition interval and run time. For this
example, set Acquisition Interval to 2 seconds and Run Length to 10 minutes.
The Logging tab allows the user to select which components will be logged as data.
Select Signal responses and Data Channel responses for this method.
Data Grid and Trend Plot allow the user to set the window size on the real-time
logging and plotting displays. Set both at 10 minutes.
Click OK on the Edit Process Monitoring Parameters screen.
Completing the method
The new method will look like Figure 20 when finished. Select File/Save to save the
new method and then File/Exit to close the window. The method is now ready to run.
24 Acquiring Data Diablo 5000A RTGA Getting Started Manual
Figure 20. The completed method with the component tree expanded.
Acquiring Data
Preparation
Select Acquisition/Manual from the menu on the top screen to open the Real Time
Gas Analyzer Manual Acquisition window (Figure 21).
Diablo 5000A RTGA Getting Started Manual Acquiring Data 25
Figure 21: the MS Sensor Manual Acquisition control panel
This example will use the method just created to acquire data from the ambient air.
The Acquisition screen will open with the currently loaded method already listed.
1. Select the button next to the Method field to choose a method to run. When the
Select Method window opens, choose the AIR.M method and select OK. AIR.M
will now appear in the Method field.
2. A folder is needed to store the acquired data. Select the button next to the Data
File field. The Select Data file window opens. Like methods, data files are
composed of several individual files in one folder. Data File folders are named
with up to eight characters ending with a .d extension.
3. To create a new data file, select the Data File field at the top of the window, type
airtest into the field and select OK.
4. Notice that the two instruments used in the method are listed in the window on
the right. 5977 and Pressure Sensor are both offline. Click Initialize Instruments
to bring the instruments online (Figure 22).
Figure 22. The control panel showing both instruments are “online”.
26 Acquiring Data Diablo 5000A RTGA Getting Started Manual
Online status means that communication has been established with the
instrument and it is ready to receive commands.
5. Click the "Initialize Acquisition" button to continue. Use the Sample
Information window (Figure 23) to describe the sample and enter related
information. Fill out the information fields as shown, then select OK
Figure 23. Entering sample information.
One window opens for each trend plot and the data grid used by the method.
Since no information is acquired yet, the trend plots and data grid are empty.
Note that the status indicators for the instruments have both changed to Ready.
The user can now size the windows according to their preference.
Hint: The easiest way to arrange the windows for a new method is to first select the
Manual Acquisition control panel window and drag it to the upper left corner of the
MS Sensor application window. Next select “Tile Horizontal” from the “Window”
menu.
Start the run
Start the run by pressing the "Start: button. Data will begin appearing in the grid and
trend plot windows and the instrument status will change to Acquiring.
Diablo 5000A RTGA Getting Started Manual Troubleshooting 27
Stop the run and view the results
A running method collects data until Stop is pressed or the run time has elapsed.
Once the method is stopped, the data can be reviewed in Excel or any other package
capable of reading a.CSV file.
The data generated in the air sample run is illustrated in Figure 24. This is the data
channel response data that was logged.
The signal channel response data is in a separate .CSV file named signals.
The data file can be accessed directly by selecting Tools/View Data File. A selection
box will be presented that allows the user to select which of the saved data (signal
results, calculation results, data channel results, or run log) to open. The data will be
displayed by the application selected in the Tools/Options menu. Alternatively, you
can open the data directory and then open the data files into a program such as
Notepad or Excel.
Figure 24. MS Sensor results displayed in Microsoft Excel.
Troubleshooting
Evaluating RTGA Interface Performance
Use the following procedure to evaluate the performance of your RTGA interface if
you think there might be a leak or plug:
28 Troubleshooting Diablo 5000A RTGA Getting Started Manual
1) First, check the interface pressure displayed on the PDR2000* pressure
controller.
With the interface exposed to ambient pressure (room air), the pressure should
be in the range of ~80-120 mTorr (0.080 to 0.120 Torr). If the pressure is
significantly higher than this, then you may have a leak in one of the interface
fittings. If the pressure is significantly lower than this, then your sample orifice
may be plugged. Proceed to the next steps to isolate and identify the problem.
*The capacitance manometer should be on for at least 4 hours before evaluating
the pressure.
2) To check for leaks in the 5975 or 5977 MSD, close the isolation valve on the
RTGA interface, and then check the pressure on the front panel display on the
MSD – press the "Menu" key until "MS parameters" is displayed and the "Item"
key until "High Vacuum Pressure" is displayed. With the isolation valve closed
and the 5975 MSD pumped down, the High Vacuum Pressure should be in the
mid to low 10^-7 Torr range. If the pressure is significantly higher than this,
then you may have a leak in the MSD or in the interface connection to the
vacuum manifold.
To confirm a leak in the MSD, run an "Air and Water Check" from the Tune
Window – make sure the isolation valve is closed and select "Air and Water
Check" from the "Tune" menu of the Tune Window. Select "Yes" to adjust to
standard values. At the bottom of the 597x Air and Water Check report, the
28/69 Nitrogen% should be <10%. If the Nitrogen% is significantly higher than
10%, then you may have a leak in the MSD.
3) To check for a leak in the RTGA interface, close the isolation valve, and plug
both arms of the sample interface "Tee" with the 1/16" caps provided in the
RTGA ship kit. If your interface is configured without a tee, then plug the inlet
with an appropriate fitting. Wait for the interface pressure on the PDR2000 to
stabilize, which may take several minutes. With the isolation valve closed and
the interface plugged, the interface pressure should be close to 0 Torr. If the
pressure stabilizes significantly higher than 0 Torr, then you may have a leak in
the interface.
To confirm a leak in the RTGA interface, run an "Air and Water Check" as
described in step 2 with the isolation valve *open* and the sample inlet plugged.
At the bottom of the 597x Air and Water Check report, the 28/69 Nitrogen%
should be <10%. If the Nitrogen% is significantly higher than 10% then you
may have a leak in one of the fittings connected to the RTGA interface.
4) To check for a plugged sample orifice, open one arm of the sample interface
"Tee" to ambient (room) air. If the interface pressure displayed on the PDR2000
is significantly below 80 mTorr (0.08 Torr), then your sample orifice may be
plugged.
To confirm a plugged sample orifice, with the isolation valve *open* and the
sample interface tee open to ambient (room) air, run an "Air and Water Check"
as described in step 2. At the bottom of the 597x Air and Water Check report,
the 28/69 Nitrogen% should be >80%. If the Nitrogen% is significantly lower
than 80% then you probably have a plugged sample orifice.
Diablo 5000A RTGA Getting Started Manual Index 29
Index
A
Acquiring Data 24
Add the additional instruments (e.g., the pressure
transducer) 18
autotune 7, 9
autotuning 9
Auto-tuning the controller 9
C
Calculations component (optional) 19
Changing Orifice Disks 6
Changing the interface temperature 8
ChemStation 1, 2, 12, 14, 18
Completing the method 23
Configuring the MS Sensor software 13
Connecting sample lines 5
Converting the MSD from RTGA to GC/MS 11
Creating a Method 14
D
data acquisition 14, 15
Data channels component 21
E
Evaluating RTGA Interface Performance 27
Excel 1, 14, 27
G
GC/MS 11
Getting Started 1
H
Hydrogen 11, 17
I
Installation 2
Instruments components 16
Introduction to creating MS Sensor Methods 14
M
Method components 15
MS Sensor Software 3
MSD ChemStation or MassHunter Acquisition
Software 2
MSD Configuration for low-mass (hydrogen) detection
11
O
orifice disks 6, 7
Overview 1
P
PDR 2000 7, 10, 18
Preparation 24
pressure sensor 1, 9, 10, 11, 18, 19
Pressure sensor operation and maintenance 9
Process monitoring parameters 22
R
RTGA Tuning Procedure: 17
S
Setting MS Sensor System Options 12
Setting the Temperature Display Units 8
Setting up the Hardware 5
Signals components 18
Special Hardware Considerations 11
Start the run 26
Starting the MS Sensor software 12
Stop the run and view the results 27
Support 2
System Installation 2
T
Temperature controller operation and maintenance 8
Theory of Operation 4
To configure the pressure sensor controller: 10
To connect the pressure sensor controller to the PC 10
To connect the pressure sensor to the cross 9
To zero the pressure sensor: 10
Troubleshooting 27
Tuning the RTGA Mass Spectrometer 17
30 Index Diablo 5000A RTGA Getting Started Manual
V
Verify the MSD ChemStation or MassHunter GC/MS
Installation 3
W
Watlow EZ-Zone Controller 8